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首页> 外文期刊>Journal of mass spectrometry: JMS >New clostebol metabolites in human urine by liquid chromatography time-of-flight tandem mass spectrometry and their application for doping control
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New clostebol metabolites in human urine by liquid chromatography time-of-flight tandem mass spectrometry and their application for doping control

机译：液相色谱飞行时间串联质谱法测定人尿中新的clostebol代谢物及其在掺杂控制中的应用

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摘要

In this study, clostebol metabolic profiles were investigated carefully. Clostebol was administered to one healthy male volunteer. Urinary extracts were analyzed by liquid chromatography quadrupole time-of-flight mass spectrometry (MS) using full scan and targeted MS/MS techniques with accurate mass measurement for the first time. Liquid-liquid extraction and direct injection were applied to processing urine samples. Chromatographic peaks for potential metabolites were found by using the theoretical [M-H](-) as target ion in full scan experiment, and their actual deprotonated ions were analyzed in targeted MS/MS mode. Fourteen metabolites were found for clostebol, and nine unreported metabolites (two free ones and seven sulfate conjugates) were identified by MS, and their potential structures were proposed based on fragmentation and metabolism pathways. Four glucuronide conjugates were also first reported. All the metabolites were evaluated in terms of how long they could be detected and S1 (4-chloro-5-androst-3-ol-17-one-3-sulfate) was considered to be the long-term metabolite for clostebol misuse detected up to 25days by liquid-liquid extraction and 14days by direct injection analysis after oral administration. Five conjugated metabolites (M2, M5, S2, S6 and S7) could also be the alternative biomarkers for clostebol misuse. Copyright (c) 2015 John Wiley & Sons, Ltd.
机译：在这项研究中，对clostebol代谢谱进行了仔细研究。将Clostebol施用给一名健康的男性志愿者。尿液提取物通过液相色谱四极杆飞行时间质谱（MS）进行分析，这是首次使用全扫描和靶向MS / MS技术进行的精确质量测量。液液萃取和直接进样用于处理尿液样品。在全扫描实验中，以理论上的[M-H]（-）作为目标离子，发现了潜在代谢物的色谱峰，并在目标MS / MS模式下分析了它们的实际去质子离子。质谱鉴定出14种代谢产物，质谱鉴定了9种未报告的代谢产物（2种游离代谢产物和7种硫酸盐结合物），并根据裂解和代谢途径提出了其潜在结构。还首次报道了四种葡糖醛酸结合物。对所有代谢物的检测时间进行了评估，并将S1（4-氯-5-androst-3-ol-17-one-3-硫酸盐）视为长期检测出的clostebol滥用的长期代谢物口服后最多25天（通过液液萃取）和14天（通过直接注射分析）。五个共轭代谢物（M2，M5，S2，S6和S7）也可能是滥用Clostebol的替代生物标志物。版权所有（c）2015 John Wiley＆Sons，Ltd.

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